Method of separating organic materials from aqueous liquids.



- To all whom it may concern.-

HENRY M GOODMAN, or LOUISVIlILLE, KnnrUcKY.

METHOD or snimmrrne onennrc mn'rnamns'rnonr AQUEOUS-LIQUIDS.

No Drawing.

. Be it known that I, HENRY a citizen of the United States, residing at Louisville, in the county of Jefferson and State of Kentucky, have invented a new and useful Method of Separating Organic Materials from Aqueous Liquids, of which the following .is a specification.

This invention relates to method ofseparating organic materials of mixed nature from distillers slop and other aqueous fluids having an acid reaction.

The invention consists in the method of operation hereinafter recited, whereby organic materials of a mixed character contained either in a state of solutionor in suspension in water or. other aqueous flulds, having an acid reaction, may be separated, removed and recovered.

The invention further consists in coagulatin the organic materials contained in "distil ersslop and other aqueous fluids, hav- I or uncoagulated,such asglobulins,

ing an acid reaction, and in the manner hereinafter recited to effect separation of such organic material and recovering the same.

The invention consists in employlng a soluble salt of ironeither with or without the aid of heat to effect the coagulation of organic'materials contained in distillers slop and other aqueous liquids, having an acid reaction, either in solution or suspension, 1n order to separate and recover same.

Other objects and purposes of the invention will appear more fully hereinafter.

A -mixture of organic materials such as various" fats or their decomposition or saponification products, proteids, coagulated vitellins, albumins, albuminates, peptones, organic acids, carbo-hydrates, and various decomposition products is generally of an acld reaction,,and the special purpose of the presentinventionis to extract, separate, or remove and recover these solids or organic materials from the Water or other aqueous fluids in which they are contained, either in a state of solution or suspension, as unaltered, pure and free a condition as 1t-1s possible to do so. This extractioncannot be accomplished by mere neutralization alone for the reason that the alkali employed to efi'ect neutralization and precipitation,

only precipitates the albuminates 1n an uncoagulated condition, and these albuminates when precipitated will again pass into solution, if the liquid from which they are be- Speeiflcation of Letters Patent. Application filed April 8, 1905. Serial No. 253,210.

M. GOODMAN,

'ing precipitated becomes too alkaline. Moreover, during the neutralization the fats contained in the aqueous fluids undergo saponification more or less complete, and the fatty acids set free combine with the alkali to form soaps, which are soluble or insoluble according to the alkali used and the many and varied reactions occurring between the alkali and the different organic substances,

= Patented Aug. 2, 1910.

all at the same time, rendering the complete extraction'of such organic materials under .thesecircumstances in an unaltered condi:

tion a practically absolute impossibility.

In accordance with this improved method and invention, no effort is made to secure neutralization in the beginning of the operation.- On the contrary and in accordance with the invention, there is added to the distillers slop or other aqueous fluid of similar character containing the, organic materials to be extracted, separated and recovered, a soluble salt of iron. It has been found that by treating distillers slop con taining the organic materials to be extracted, and having an acid reaction, with a soluble iron salt, coagulation of the organic mate rials contained in the aqueous 'fluid under treatment begins at once. It has been found in practice that any soluble salt of iron may be employed for the pur ose of coagulating all the roteids oontaine in the acid liquid that wi l coagulate from the acid menstruum under the actionof the iron salt, andsuccess has been attained by emplo ing for this purpose ferrous or ferric sul ate, chlorid, nitrate, or acetate, and by reason of the cheapness and greater efficiency it is preferable to employ one or theother of these salts of iron, and in the order named, and in the proportion of about thirty drops to a teaspoonful, more or less, of a saturated solution of the iron salt, including Monsels solution to one gallon of aqueous fluid such as distillers slop or the Waste liquor pressed from brewers" spent grains. It has also been found that the coagulation of the organic materials contained in the aqueous fluid to which the soluble iron has been added is materially aided, if the liquid is treated while hot or if cold, heating the liquid to a temperature between 160 and 212 Fahr.

The coagulation of the albuminous organic matters bythe iron salt is just as ronounced' if the di'stille'rs slop is treated in the cold but the time required is longer, whereas if the liquid is Warmedthe separaat this appliances. The coagulum recovered by the addition of the iron salt amounts to between three to four and one half ounces per gallon and is composed of proteids in organic combination with the iron, and fats. This constitutes the first step of this improved process and if by reason of the expense involved it becomes desirable to stop oint the filtrate may be thrown away. fter the removal of the coagulum produced by the addition of the iron salt to the distillers slop, having an acid reaction, a considerable amount of proteid material and fats is still retained in the aqueous fluid, amounting to from a to 1 ounce per gallon. Another portion of the iron salt may then be added to the acid filtrate, obtained from the first step, and this fluid neutralized by the addition of an alkali, and in about the roportion of four pounds, more or less 0 the alkali, as caustic potash, or soda or lime to 1,000 gallons of the aqueous fluids, as distillers slop or the waste liquids from brewers spent grains.

Neutralization of the acid filtrate left after the first addition of the iron salt causes precipitation of the remaining proteid materials, but the addition of the lI'OIl salt previous to neutralization causes an alteration of the proteid molecule and the percipita tion of the proteid materials under such circumstances is more prompt and permanent. The precipitate so formed can now be removed and recovered by filtration or decantation. This constitutes the second and final step of this improved process. The strongly acid filtrate remaining after the first step.

is still cloudy whereas the neutral or faintly acid or faintly alkaline filtrate remaining after the second step is as clear as sprin water and shows entire removal of proteid material, except erhaps the presence of an exceedingly smal amount of peptone or albumoses as shown by a delicate response to the Bieuret reaction.

From the foregoing description, it will be seen that the soluble molecules ofthe albuminous organic materials contained in the acid distillers slop become altered by the use and action of the iron salt, in the first step producing a true coagulation of the proteid material from the acid liquid, and

in the second step enabling the alkali toform a more permanent percipitate from the acid fluid.

The process above described, while applicable generally to any waste liquids, having an acid rwction, holding in solution or suspension the solid materials herein above set forth, is particularly adapted to the treatment of distillery slop and may be applied to the liquid pressed out of brewers spent grains, the liquid left in glucose refuse, starch refuse, and the liquid pressed from cossettes or beet pulps. The process may be applied to distillery slop before the removal of the solid remnants of grain by means of filter presses, roller presses, or other mechanical devices, but it is preferred to apply the process to the liquid at present passing the sieves and the presses, and which is ordinarily either thrown away or sold to dairymen as food for cattle. This liquid contains the most valuable portion of the nutriment and it is to this liquid that this method is applied in order to recover this additional nutriment in a dry state, in

which form it is especially valuable as a food for dairy cattle, as it adds a value of from 30 to 40 per cent. to the dried grains at present extracted from distillery slop. The organic matter extracted by the above process consists almost entirely of coagulated proteids and fats, and by adding this material 'to' the grains at present extracted from distillery slop by the present purely mechanical processes, there is added not only to the nutritive value of the dried grains, but the amount of material recovered ,1

is greatly increased.

Repeated experiment has demonstrated and has conclusively shown that only so much of the soluble iron salt (from to 1 teaspoonful of a saturated solution, or its equivalent, to one gallon of distille' slop, or one gallon of the liquid presse from brewers spent grains) ulate the coagulable a buminous matters contained in the acid liquid. Any excess of the iron salt above the said quantity does not cause coagulation of the entire amount of the albuminous organic matters in the acid solution. amount of the iron salt is used, or if just suflicient is used to coagulate all of the coagulable organic mattersin the acid solution, tests ap lied to the filtrate will not demonstrate the presence of the iron salt. Whereas, if an excess of the iron salt'be used over and above the amount required to coagulate the coagulable organic matters contained in a given amount of the acid slop, then chemical tests applied to the acid filtrate will demonstrate iron remaining in solution in the filtrate. It is therefore evident that in the first step only a certain amount of the albuminous organic matters in the acid solution becomes coagulable under the influence of the iron salt. The albuminous matters remaining in solution after the coagulable albumins (rendered is necessary to coag- If less than the necessary the remaining albuminous organ c matters,

7 resembling in many respects a true coagulation.

What is claimed as new is- 1. The method of separating albuminous organic materials from distillers slop having an acid reaction which consists in coagulating the albuminous organic materials contained therein and removing part of the albuminous materials therefrom, then adding a soluble salt of iron thereby forming a permanent precipitate of the remaining albuminous matters, then neutralizing the solution with an alkali and separating the coagulum and recovering the same.

2. The method of separating organic materials from distillers slop having an acid reaction which consists in coagulating a portion of the albuminous organic materials thereof by the addition to such fluids of a" y then separating and resoluble salt of iron,

covering the resultant coagulum by filtering the mass, then again treating the filtrate with a soluble salt of iron whereby a further proportion of the albuminous organic materials will be coagulated and finally separating and recovering the second resultant coagulum.

The method of separating albuminous organic materials from distillers slop having an acid reaction which consists in coagulating part of albuminous organic materials contained therein by the addition to such fluid of a soluble salt of iron, filtering and recovering the coagulum, then adding a second portion of the soluble iron salt to the acid filtrate, then neutralizing and thereby precipitating the albuminous organic'materials, then filtering and recovering the final coagulum.

In witness whereof, I have hereunto set my hand this 20th day of March, 1905, in the presence of the subscribing witnesses.

HENRY M. GOODMAN. Witnesses:

HUGHES MoonE, J. W. BILES. 

